CN112844348A - TiO with micro-nano structure2Preparation method of nanotube array photo-anode - Google Patents
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- 239000002071 nanotube Substances 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000002086 nanomaterial Substances 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 15
- 238000000137 annealing Methods 0.000 claims abstract description 11
- 238000010329 laser etching Methods 0.000 claims abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001301 oxygen Substances 0.000 claims abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 9
- 229910003087 TiOx Inorganic materials 0.000 claims abstract description 4
- 238000005530 etching Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 19
- 239000010936 titanium Substances 0.000 claims description 16
- 239000012153 distilled water Substances 0.000 claims description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 12
- 229910052719 titanium Inorganic materials 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000003792 electrolyte Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 7
- 238000003491 array Methods 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 45
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 20
- 238000005215 recombination Methods 0.000 abstract description 4
- 230000006798 recombination Effects 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- 238000012360 testing method Methods 0.000 description 5
- 229910021607 Silver chloride Inorganic materials 0.000 description 4
- 238000007743 anodising Methods 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 206010021143 Hypoxia Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000001075 voltammogram Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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Abstract
The invention provides TiO with a micro-nano structure2The preparation method of the nanotube array photo-anode comprises the following steps: (1) preparation of amorphous TiO by anodic oxidationxA nanotube array; (2) will not shape TiOxPerforming laser etching on the nanotube array under laser irradiation to obtain TiO with a micro-nano structure and oxygen defectsxA nanotube array; (3) TiO with micro-nano structure and oxygen defectxAnnealing the nanotube array to obtain the TiO with the micro-nano structure2Nanotube array photoanode. The method of the invention utilizes a laser etching method to etch TiO2The surface of the nanotube is treated to increaseTiO is2Effective area and surface active site of nanotube, and treated TiO2The hydrophilicity of the nanotube array is obviously improved, so that the carrier recombination rate is reduced, and the photoelectric catalysis efficiency is increased.
Description
Technical Field
The invention relates to the technical field of photoelectrochemistry and photoanode materials, in particular to TiO with a micro-nano structure2A method for preparing a nanotube array photo-anode.
Background
Titanium dioxide is a multifunctional material that is chemically stable, strong (large surface area) and has high photocatalytic activity as well as high dielectric constant and low production cost, while it has a wide range of potential applications, including for example in solar cells, photocatalysts and water splitting and gas sensors, among others. Nevertheless, TiO2The intrinsic band gap of a nanotube limits its absorption in the ultraviolet region of the solar spectrum. In addition, the rapid recombination of the photo-generated electrons and holes greatly reduces the quantum efficiency and the efficiency of the photoelectrocatalytic decomposition of water. Therefore, how to improve the charge separation efficiency and enhance the visible light catalytic activity has become a practical problem to be solved. For this purpose, the invention provides a method for etching TiO by laser2Preparation of TiO with oxygen deficiency by nanotube array2A novel method of nanotube arrays that addresses TiO2The problem of high recombination rate of carriers effectively improves the photoelectric catalytic performance of the photocatalyst and obtains larger photocurrent.
Disclosure of Invention
The invention aims to provide TiO with a micro-nano structure2A method for preparing a nanotube array photoanode, which solves the problem of TiO prepared by the prior art2The effective area and the surface active sites of the nano tube are few, and the photoelectrocatalysis performance is low.
The above purpose of the invention is realized by the following technical scheme:
TiO with micro-nano structure2The preparation method of the nanotube array photo-anode comprises the following steps:
(1) preparation of amorphous TiO by anodic oxidationxA nanotube array;
(2) will not shape TiOxPerforming laser etching on the nanotube array under laser irradiation to obtain TiO with a micro-nano structure and oxygen defectsxA nanotube array;
(3) TiO with micro-nano structure and oxygen defectxAnnealing the nanotube array to obtain the TiO with the micro-nano structure2Nanotube array photoanode.
In the present invention, amorphous TiOxThe parameters of the nanotube array for laser etching under laser irradiation are set as follows: the laser frequency is 100-200kHz, the marking speed is 500-1500mm/s, and the pulse width is 1-10ns during etching, and the etching power adjustment range is 3-18W.
Preferably, the etching power is set to be 3-18W under the conditions that the laser frequency is 200kHz, the marking speed is 1500mm/s and the pulse width is 10 ns.
In the invention, the annealing treatment is carried out by raising the temperature to 400-600 ℃ at the temperature raising rate of 1-5 ℃/min for 1-5 h.
Preferably, the annealing treatment is carried out by raising the temperature to 500 ℃ at a temperature raising rate of 2 ℃/min for 2 h.
In the invention, the amorphous TiO is prepared by adopting an anodic oxidation methodxThe process of nanotube arrays is as follows: the titanium sheet is put into an electrolytic bath prepared by glycol, ammonium fluoride and distilled water for anodic oxidation.
Preferably, the mass volume ratio of the ammonium fluoride to the distilled water in the electrolyte is 0.072:1 (g/ml); the volume ratio of ethylene glycol to distilled water was 20: 1.
Further, the voltage of the anodic oxidation is 40-70V, and the anodic oxidation time is 1-5 hours.
Preferably, the anodizing voltage is 60V and the anodizing time is 90 min.
In the invention, before the titanium sheet is subjected to anodic oxidation, acetone, ethanol and distilled water are sequentially used for carrying out ultrasonic cleaning on the titanium sheet.
Compared with the prior art, the invention has the following beneficial effects:
(1) the method of the invention utilizes a laser etching method to etch TiO2The surface of the nano tube is treated to increase TiO2Effective area and surface active site of nanotube, and treated TiO2The hydrophilicity of the nanotube array is obviously improved, so that the carrier recombination rate is reduced, and the photoelectric catalysis efficiency is increased.
(2) The invention is realized by etching the TiO2The nanotube array is annealed, which results in TiO2The crystallinity is increased, thereby improving the photoelectrocatalysis performance of the material.
Drawings
FIG. 1 shows TiO prepared in example 3 of the present invention2XRD pattern of nanotube array photo-anode;
FIG. 2 shows TiO prepared in example 3 of the present invention2SEM image of nanotube array photo-anode;
FIG. 3 shows TiO prepared in example 3 of the present invention2A water contact angle test chart of the nanotube array photoanode;
FIG. 4 is a water contact angle test chart of Ti material;
FIG. 5 is TiO2A water contact angle test chart of the nanotube array;
FIG. 6 shows TiO prepared in example 3 of the present invention2And (3) testing the photocurrent of the nanotube array photoanode.
Detailed Description
The present invention is further described below in conjunction with specific examples to better understand and implement the technical solutions of the present invention for those skilled in the art.
Example 1
TiO with micro-nano structure2The preparation method of the nanotube array photo-anode comprises the following steps:
(1) the titanium sheet (length: 5cm, width: 1cm) was ultrasonically cleaned with acetone, ethanol, and distilled water for 30min, respectively. 5ml of distilled water were weighed into a reaction vessel and 0.36g of NH were added simultaneously4F (ammonium fluoride) was dissolved and then 100ml (CH) was weighed2OH)2(ethylene glycol) is poured into the mixed solution and evenly stirred to prepare electrolyte; placing a titanium sheet in the prepared electrolyteAnodizing at 60V voltage for 90min to prepare amorphous TiO2Nanotube array (TiO)xNanotube arrays). After being washed clean, the mixture is placed in an oven at 60 ℃ for drying.
(2) The amorphous TiO obtained in the step (1)2Setting the etching power of the nanotube array to 9W for laser etching under the conditions that the fixed etching frequency is 200kHz, the fixed marking speed is 1500mm/s and the fixed pulse width is 10ns to obtain etched TiO2Nanotube of TiO with micro-nano structure and oxygen defectxAn array of nanotubes.
(3) Etching the TiO obtained in the step (2)2Heating the nanotube in a muffle furnace at a heating rate of 2 ℃/min to 500 ℃ and annealing for 2h to obtain TiO with a micro-nano structure2Nanotube array photoanode.
With the TiO thus prepared2The nanotube array photoanode is a working electrode (area of 1cm)2) Platinum electrode as auxiliary electrode, Ag/AgCl electrode as reference electrode, 0.5mol/L NaSO4The solution is electrolyte, the photoelectrochemical type performance is tested under a sunlight simulator (the light intensity of 1 sun), and the bias voltage is 1.2V, so that 0.275mA/cm is obtained2A photocurrent.
Example 2
TiO with micro-nano structure2The preparation method of the nanotube array photo-anode comprises the following steps:
(1) the titanium sheet (length: 5cm, width: 1cm) was ultrasonically cleaned with acetone, ethanol, and distilled water for 30min, respectively. 5ml of distilled water were weighed into a reaction vessel and 0.36g of NH were added simultaneously4F (ammonium fluoride) was dissolved and then 100ml (CH) was weighed2OH)2(ethylene glycol) is poured into the mixed solution and evenly stirred to prepare electrolyte; placing the titanium sheet in prepared electrolyte, and anodizing for 90min at the voltage of 60V to prepare the amorphous TiO2Nanotube array (TiO)xNanotube arrays). After being washed clean, the mixture is placed in an oven at 60 ℃ for drying.
(2) The amorphous TiO obtained in the step (1)2The nanotube array has a fixed etching frequency of 200kHz, a fixed marking speed of 1500mm/s and a fixed pulse width of 10nsSetting the etching power to 9W for laser etching to obtain etched TiO2Nanotube of TiO with micro-nano structure and oxygen defectxAn array of nanotubes.
(3) Etching the TiO obtained in the step (2)2Heating the nanotube in a muffle furnace at a heating rate of 2 ℃/min to 500 ℃ and annealing for 2h to obtain TiO with a micro-nano structure2Nanotube array photoanode.
With the TiO thus prepared2The nanotube array photoanode is a working electrode (area of 1cm)2) Platinum electrode as auxiliary electrode, Ag/AgCl electrode as reference electrode, 0.5mol/L NaSO4The solution is electrolyte, the photoelectrochemical type performance is tested under a sunlight simulator (the light intensity of 1 sun), and the bias voltage is 1.2V, so that 0.35mA/cm is obtained2A photocurrent.
Example 3
TiO with micro-nano structure2The preparation method of the nanotube array photo-anode comprises the following steps:
(1) the titanium sheet (length: 5cm, width: 1cm) was ultrasonically cleaned with acetone, ethanol, and distilled water for 30min, respectively. 5ml of distilled water were weighed into a reaction vessel and 0.36g of NH were added simultaneously4F (ammonium fluoride) was dissolved and then 100ml (CH) was weighed2OH)2(ethylene glycol) is poured into the mixed solution and evenly stirred to prepare electrolyte; placing the titanium sheet in prepared electrolyte, and anodizing for 90min at the voltage of 60V to prepare the amorphous TiO2Nanotube array (TiO)xNanotube arrays). After being washed clean, the mixture is placed in an oven at 60 ℃ for drying.
(2) The amorphous TiO obtained in the step (1)2Setting the etching power of the nanotube array to be 3-18W for laser etching under the conditions that the fixed etching frequency is 200kHz, the fixed marking speed is 1500mm/s and the fixed pulse width is 10ns, and obtaining etched TiO2Nanotube of TiO with micro-nano structure and oxygen defectxAn array of nanotubes.
(3) Etching the TiO obtained in the step (2)2Heating the nanotube in a muffle furnace at a heating rate of 2 ℃/min to 500 ℃ and annealing for 2h to obtain the nano-nano junctionStructural TiO2Nanotube array photoanode.
TiO prepared in this example2The XRD pattern and SEM pattern of the nanotube array photoanode are shown in figure 1 and figure 2, and the contact angle test conditions are shown in figures 3-5, namely water drops on Ti and TiO respectively2Nanotube array and TiO2The contact angle of the Ti plate is 60.89 degrees and the contact angle of the Ti plate is measured by a photo of the contact angle on the surface of the nano tube array photo anode2The contact angle of the nanotube array is 18.70 degrees, and the TiO is treated by etching2The nanotube array contact angle was 5.98 °. Thus, it can be shown that the TiO prepared according to the invention2The nanotube array photoanode has good hydrophilicity, so that the adsorption of water on the surface of the catalyst is facilitated, and a larger photocurrent is obtained.
With the TiO thus prepared2The nanotube array photoanode is a working electrode (area of 1cm)2) The platinum electrode is an auxiliary electrode, the Ag/AgCl electrode is a reference electrode, and the concentration of the platinum electrode and the Ag/AgCl electrode is 0.5mol/LNaSO4The solution is electrolyte, the photoelectrochemical performance is tested under a sunlight simulator (the light intensity of 1 sun), and a linear scanning voltammogram under the bias of 1.2V is shown in a figure 6. As can be seen from FIG. 6, the photocurrent density increased with the increase of the etching power, and the photocurrent density decreased after the power exceeded 15W, which is the optimum value for the etching power of 15W. Specifically, under other fixed conditions and a bias voltage of 1.2V, the maximum photocurrent of 0.493mA/cm is obtained when the etching power is 15W2。
The above embodiments illustrate various embodiments of the present invention in detail, but the embodiments of the present invention are not limited thereto, and those skilled in the art can achieve the objectives of the present invention based on the disclosure of the present invention, and any modifications and variations based on the concept of the present invention fall within the scope of the present invention, which is defined by the claims.
Claims (10)
1. TiO with micro-nano structure2The preparation method of the nanotube array photo-anode is characterized by comprising the following steps of:
(1) by using yangPreparation of amorphous TiO by polar oxidationxA nanotube array;
(2) will not shape TiOxPerforming laser etching on the nanotube array under laser irradiation to obtain TiO with a micro-nano structure and oxygen defectsxA nanotube array;
(3) TiO with micro-nano structure and oxygen defectxAnnealing the nanotube array to obtain the TiO with the micro-nano structure2Nanotube array photoanode.
2. The micro-nano structured TiO of claim 12The preparation method of the nanotube array photoanode is characterized in that the amorphous TiO isxThe parameters of the nanotube array for laser etching under laser irradiation are set as follows: the laser frequency is 100-200kHz, the marking speed is 500-1500mm/s, and the pulse width is 1-10ns during etching, and the etching power adjustment range is 3-18W.
3. The micro-nanostructured TiO according to claim 22The preparation method of the nanotube array photoanode is characterized in that the etching power is set to be 3-18W under the conditions that the laser frequency is 200kHz, the marking speed is 1500mm/s and the pulse width is 10 ns.
4. TiO with micro-nano structure according to any one of claims 1 to 32The preparation method of the nanotube array photoanode is characterized in that the annealing treatment is carried out by heating to 400-600 ℃ at a heating rate of 1-5 ℃/min for annealing for 1-5 h.
5. The TiO with micro-nano structure of claim 42The preparation method of the nanotube array photoanode is characterized in that the annealing treatment is carried out by heating to 500 ℃ at a heating rate of 2 ℃/min for 2 h.
6. The TiO with micro-nano structure of claim 42The preparation method of the nanotube array photoanode is characterized in that the amorphous TiO is prepared by adopting an anodic oxidation methodxThe process of nanotube arrays is as follows: the titanium sheet is put into an electrolytic bath prepared by glycol, ammonium fluoride and distilled water for anodic oxidation.
7. The TiO with micro-nano structure of claim 62The preparation method of the nanotube array photoanode is characterized in that the mass volume ratio of ammonium fluoride to distilled water in electrolyte is 0.072:1 (g/ml); the volume ratio of ethylene glycol to distilled water was 20: 1.
8. TiO with micro-nano structure according to claim 6 or 72The preparation method of the nanotube array photoanode is characterized in that the voltage of anodic oxidation is 40-70V, and the time of anodic oxidation is 1-5 hours.
9. The micro-nanostructured TiO according to claim 82The preparation method of the nanotube array photoanode is characterized in that the voltage of anodic oxidation is 60V, and the anodic oxidation time is 90 min.
10. The micro-nanostructured TiO according to claim 82The preparation method of the nanotube array photoanode is characterized in that acetone, ethanol and distilled water are sequentially used for carrying out ultrasonic cleaning on a titanium sheet before the titanium sheet is subjected to anodic oxidation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114042187A (en) * | 2021-09-18 | 2022-02-15 | 广东省华源康泰生物科技有限责任公司 | Preparation method of micro-area titanium oxide nanotube structure bone dental implant material |
| CN114188063A (en) * | 2021-12-13 | 2022-03-15 | 中国核动力研究设计院 | Nanotube array-based Schottky junction, preparation method thereof and beta nuclear battery |
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